CN102534333A - Method for preparing fine-grain high-density TZM (Titanium-Zirconium-Molybdenum Allo) alloy - Google Patents
Method for preparing fine-grain high-density TZM (Titanium-Zirconium-Molybdenum Allo) alloy Download PDFInfo
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- CN102534333A CN102534333A CN2012100014096A CN201210001409A CN102534333A CN 102534333 A CN102534333 A CN 102534333A CN 2012100014096 A CN2012100014096 A CN 2012100014096A CN 201210001409 A CN201210001409 A CN 201210001409A CN 102534333 A CN102534333 A CN 102534333A
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Abstract
The invention discloses a method for preparing a fine-grain high-density TZM (Titanium-Zirconium-Molybdenum Allo) alloy. The method disclosed by the invention comprises the following steps of: with pure molybdenum powder, ZrH2 powder, La2O3 powder and graphite powder as raw materials, mixing the raw materials, and carrying out ball milling, press molding, presintering and high-temperature sintering to obtain the TZM alloy. The TZM alloy prepared by using the method disclosed by the invention has the characteristics of fine crystal grains, distribution uniformity, low porosity, high compactness, simple preparation process and strong operability and controllability and has the most remarkable advantages that: on the basis of the traditional ZTM alloy preparation method, rare earth oxide La2O3 is solid-solid doped in the alloy powders, a mode of combining mixing and ball-milling of the alloy powders and a mode of sectional sintering during high-temperature sintering are adopted, crystal grains are fined, the alloy density is remarkably improved, the sintering temperature of the TZM alloy is reduced to 1800-2000 DEG C from 2100-2300 DEG C in the traditional method, therefore energy resources are saved and requirements of an enterprise on the fine-grain TZM alloy material with high density can be met.
Description
Technical field
The invention belongs to and adopt powder metallurgy process to prepare the refractory metal alloy field, relate to the preparation of TZM alloy, particularly a kind of method for preparing thin brilliant high-compactness TZM alloy.
Background technology
Molybdenum alloy is to be that matrix adds the non-ferrous alloy that other element constitutes with the molybdenum.Owing to have the excellent high-temperature mechanical property, be the molybdenum alloy of representative with TZM (Titanium-Zirconium-Molybdenum Allo), can be widely used in fields such as aerospace industry, nuclear power industry and electronic industry.Preparation TZM alloy mainly adopts smelting process and powder metallurgic method at present.Smelting process is that elements such as pure molybdenum and a certain amount of Ti, Zr are carried out melting under vacuum or protection of inert gas, adopts modes such as casting and mechanical workout to make the TZM blank then.Powder metallurgic method is with high pure molybdenum powder and TiH
2Powder, ZrH
2Uniform mixing is after isostatic cool pressing or compression molding in proportion for powder and spraying carbon black powder, and high temperature sintering under protective atmosphere obtains the TZM blank then.Adopt powder metallurgic method to prepare the TZM alloy and can save main equipments such as vacuum consumable electrode arc furnace and extrusion machine, the explained hereafter cycle is short, consume low, throughput and yield rate height, cost reduces greatly.
The problem that exists for TZM alloy technology of preparing at present is that crystal grain is thick, and porosity is big, and alloy density is lower, has influenced the mechanical property of TZM alloy.Rare earth doped oxide compound is refinement TZM alloy grain and the effective ways that improve its density.Because the rare earth oxide particle is distributed in the surface of molybdenum powder as second-phase dispersion, to molybdenum crystal grain original grain boundary forming core in the sintering process with grown up inhibition, the inhibition grain growth; The diffusion of material and flow is fully carried out during high temperature sintering, and the rare earth oxide of disperse is particle-filled in the sintering hole, and sintering TZM alloy density is increased.
The key of rare earth doped oxide compound is the control of rare earth oxide distributing homogeneity, and the advantage of rare earth doped oxide compound is simple to operate, and doping is easy to control, and doping process is the easiest, and facility investment is few, is easy to tissue production.
Summary of the invention
Defective or deficiency to above-mentioned prior art exists the objective of the invention is to, and propose a kind of method for preparing thin brilliant high-compactness TZM alloy.This method has been prepared rare earth doped oxide compound La with powder metallurgical technique
2O
3The TZM alloy, satisfy the demand of enterprise to thin crystalline substance, high-compactness TZM alloy material.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of method for preparing thin brilliant high-compactness TZM alloy is characterized in that, specifically prepares process and may further comprise the steps successively:
Step 1, material choice:
Molybdenum powder: purity>=99.96%, loose density 0.95g/cm
3~1.40g/cm
3, granularity 2.0 μ m~3.5 μ m;
La
2O
3Powder: purity is 99.99%, and granularity is 0.5 μ m~2 μ m;
The TiH powder: purity >=99.5%, granularity are 5~8 μ m;
ZrH
2Powder: purity>=99.5%, granularity are 5~8 μ m;
Graphite Powder 99: purity >=99.5%, maximum particle size are no more than 10 μ m;
Step 2 is carried out proportioning: TiH according to following mass percent
2Powder: 0.45%~0.65%, ZrH
2Powder: 0.06%~0.14%, Graphite Powder 99: 0.02%~0.06%, La
2O
3Powder: 0.5~1.5%, surplus is a molybdenum powder, the per-cent sum of raw material is 100%;
Step 3 is packed each raw material of formula ratio in the three-dimensional blender machine into, mixes 1~4 hour the powdered alloy that obtains mixing with rotating speed 30r/min~60r/min;
Step 4 is packed powdered alloy into and is carried out ball milling in the ball mill, and drum's speed of rotation is 30r/min~200r/min, and being placed with diameter in the ball mill is the molybdenum ball of 10mm, and the mass ratio of molybdenum ball and powdered alloy is 2: 1,2 hours~24 hours ball milling time;
Step 5, the alloy powder behind the ball milling adopt mold pressing or isostatic pressing method to be pressed into blank, and pressure is 20Mpa~200Mpa, and the dwell time is 5s~60s;
Step 6 is carried out pre-burning with the blank that suppresses, and protective atmosphere is vacuum, hydrogen or rare gas element, and pre-sintering temperature is 1000 ℃~1200 ℃, is incubated 1 hour~4 hours;
Step 7 is carried out high temperature sintering with the blank after the pre-burning, and protective atmosphere is vacuum, hydrogen or rare gas element, and the highest sintering temperature is 1800 ℃~2000 ℃; High temperature sintering adopts the staged sintering processing; When promptly being heated to 1200 ℃~1500 ℃; Whenever at a distance from 100 ℃ of insulations 2~3 hours, when being heated to 1500 ℃~1800 ℃, whenever at a distance from 150 ℃ of insulations 2~4 hours; Be incubated 5-8 hour down at 1800 ℃~2000 ℃ at last, promptly obtain thin brilliant high-compactness TZM alloy.
The method of the thin brilliant high-compactness TZM alloy of preparation of the present invention is compared with existing TZM alloy technology of preparing, has following advantage:
1, on the basis of prior powder metallurgy, passes through rare earth doped oxide compound La
2O
3Powder, crystal grain thinning makes that the TZM alloy grain of preparation is tiny.
2, the powdered alloy hybrid mode that adopts batch mixing to combine with ball milling, ball milling make rare earth doped oxide compound La
2O
3Powder is broken repeatedly and mix, and the powder particle refinement, is evenly distributed, and good fluidity reaches the purpose of alloying element homogenizing simultaneously, has also solved solid rare earth doped oxide compound La
2O
3The uppity problem of homogeneity.
3, high temperature sintering adopts the staged sintering processing, has suppressed too growing up of TZM alloy grain, makes the gaseous impurities in the sintered blank have adequate time to evaporate simultaneously, has reduced the porosity of preparation TZM alloy, significantly improves the density of preparation TZM alloy.
4, TZM alloy sintering temperature is reduced to 1800 ℃~2000 ℃, save energy from traditional 2100 ℃~2300 ℃.
Description of drawings
Fig. 1 is the metallograph of embodiment 1 gained TZM alloy.
Fig. 2 is the metallograph of embodiment 2 gained TZM alloys.
Fig. 3 is the stereoscan photograph of embodiment 3 gained TZM alloys.
Fig. 4 is the stereoscan photograph of embodiment 4 gained TZM alloys.
The present invention is described in further detail below in conjunction with embodiment that accompanying drawing and inventor provide.
Embodiment
In following embodiment, selected raw material is the common used in industry raw material, wherein, and molybdenum powder purity>=99.96%, loose density 0.95g/cm
3~1.40g/cm
3La
2O
3The purity of powder is 99.99%; TiH powder and ZrH
2The purity of powder>=99.5%; The purity of Graphite Powder 99>=99.5%.
Below be the embodiment that the contriver provides, the invention is not restricted to these embodiment.
Embodiment 1:
Raw material: the molybdenum powder granularity is 2 μ m, TiH
2Powder and ZrH
2The granularity of powder is 5 μ m, the granularity 10 μ m of Graphite Powder 99, La
2O
3The granularity of powder is 0.5 μ m.
Carry out alloyage powder: TiH according to following mass percent
2: 0.45%, ZrH
2: 0.06%%, Graphite Powder 99: 0.05%, La
2O
3Powder is 0.5%, and molybdenum powder supplies 100%;
According to prescription powdered alloy is packed into and to mix 2 hours mixer rotating speed 30r/min, the powdered alloy that obtains mixing in the three-dimensional blender machine.
The powdered alloy that mixes packed into carry out ball milling in the ball mill, drum's speed of rotation is 50r/min, places the molybdenum ball of diameter 10mm in the ball mill, and the mass ratio of molybdenum ball and powdered alloy is 2: 1, and the ball milling time is 2 hours.
Alloy powder behind the ball milling adopts die forming, and pressure is 50Mpa, and the dwell time is 10s.
Then the blank that suppresses is carried out pre-burning, protective atmosphere is a vacuum, and pre-sintering temperature is 1000 ℃, is incubated 1 hour.
Then the blank after the pre-burning is carried out high temperature sintering, protective atmosphere is a vacuum, and the highest sintering temperature is 1800 ℃; Adopt the staged sintering processing, when being heated to 1200 ℃, whenever at a distance from 100 ℃ of insulations 2 hours; When being heated to 1500 ℃, whenever, be incubated 8 hours down at 1800 ℃ at last at a distance from 150 ℃ of insulations 2 hours.The metallograph of prepared thin brilliant high-compactness TZM alloy is shown in accompanying drawing 1.
Embodiment 2:
Raw material: the granularity of molybdenum powder is 3.5 μ m, TiH
2And ZrH
2The granularity of powder is 8 μ m, Graphite Powder 99 granularity 6 μ m, La
2O
3Powder size is 0.5 μ m.
Carry out alloyage powder: TiH according to following mass percent
2: 0.65%, ZrH
2: 0.14%, Graphite Powder 99: 0.06%, La
2O
3Powder: 1.5%, molybdenum powder supplies 100%;
The powdered alloy for preparing packed into mixed 4 hours mixer rotating speed 60r/min, the powdered alloy that obtains mixing in the three-dimensional blender machine.
The powdered alloy that mixes packed into carry out ball milling in the ball mill, drum's speed of rotation is 200r/min, places the molybdenum ball of diameter 10mm in the ball mill, and the mass ratio of molybdenum ball and powdered alloy is 2: 1, and the ball milling time is 24 hours.
Alloy powder behind the ball milling adopts the isostatic pressing method press forming, and pressure is 200Mpa, and the dwell time is 60s.
Then the blank that suppresses is carried out pre-burning, protective atmosphere is a hydrogen, and pre-sintering temperature is 1200 ℃, is incubated 4 hours.
Carry out high temperature sintering then, protective atmosphere is a hydrogen, and the highest sintering temperature is 2000 ℃; Adopt the staged sintering processing, when being heated to 1500 ℃, whenever at a distance from 100 ℃ of insulations 3 hours; When being heated to 1800 ℃, whenever, be incubated 5 hours down at 2000 ℃ at last at a distance from 150 ℃ of insulations 4 hours.The metallograph of prepared thin brilliant high-compactness TZM alloy is shown in accompanying drawing 2.
Embodiment 3:
Raw material: the molybdenum powder granularity is 3 μ m, TiH
2And ZrH
2The granularity of powder is 7 μ m, Graphite Powder 99 granularity 8 μ m, La
2O
3Powder size is 1 μ m.
Carry out alloyage powder: TiH according to following mass percent
2: 0.5%, ZrH
2: 0.09%, Graphite Powder 99: 0.05%, La
2O
3Powder: 1%, molybdenum powder supplies 100%.
The powdered alloy for preparing packed into mixed 3 hours mixer rotating speed 50r/min, the powdered alloy that obtains mixing in the three-dimensional blender machine.
The powdered alloy that mixes packed into carry out ball milling in the ball mill, drum's speed of rotation is 100r/min, places the molybdenum ball of diameter 10mm in the ball mill, and the mass ratio of molybdenum ball and powdered alloy is 2: 1, and the ball milling time is 24 hours.
Adopt the compression molding powder pressing that ball milling is good, pressure is 100Mpa, and the dwell time is 30s.
Then the blank that suppresses is carried out pre-burning, protective atmosphere is a rare gas element, and pre-sintering temperature is 1100 ℃, is incubated 3 hours.
Carry out high temperature sintering then, protective atmosphere is a hydrogen, and the highest sintering temperature is 1900 ℃; Adopt the staged sintering processing; Every when being heated to 1200 ℃ at a distance from 100 ℃ of insulations 2 hours, every during 1700 ℃ of heating at a distance from 150 ℃ of insulations 3 hours, under 1900 ℃, be incubated 6 hours at last.The stereoscan photograph of prepared thin brilliant high-compactness TZM alloy is shown in accompanying drawing 3.
Embodiment 4:
Raw material: the granularity of molybdenum powder is 2.5 μ m, TiH
2And ZrH
2The granularity of powder is 6 μ m, the granularity 6 μ m of Graphite Powder 99, La
2O
3Powder size is 1.5 μ m.
Carry out alloyage powder: TiH according to following mass percent
2: 0.55%, ZrH
2: 0.11%, Graphite Powder 99: 0.06%, La
2O
3Powder: 1.2%, molybdenum powder supplies 100%.
The powdered alloy for preparing packed into mixed 2 hours in the three-dimensional blender machine, rotating speed 50r/min makes doping La
2O
3The TZM powdered alloy of powder mixes.
The powdered alloy that mixes packed into carry out ball milling in the ball mill, drum's speed of rotation is 150r/min, places the molybdenum ball of diameter 10mm in the ball mill, and the mass ratio of molybdenum ball and powdered alloy is 2: 1, and the ball milling time is 20 hours.
Adopt the isostatic pressing method powder pressing that ball milling is good, pressure is 180Mpa, and the dwell time is 50s.
Then the blank that suppresses is carried out pre-burning, protective atmosphere is a vacuum, and pre-sintering temperature is 1100 ℃, is incubated 2 hours.
Carry out high temperature sintering then, protective atmosphere is a hydrogen, and the highest sintering temperature is 1950 ℃; Adopt the staged sintering processing, when being heated to 1300 ℃, whenever at a distance from 100 ℃ of insulations 2 hours; When being heated to 1750 ℃, whenever, be incubated 5 hours down at 1950 ℃ at last at a distance from 150 ℃ of insulations 3 hours.The stereoscan photograph of prepared thin brilliant high-compactness TZM alloy is shown in accompanying drawing 4.
Claims (1)
1. a method for preparing thin brilliant high-compactness TZM alloy is characterized in that, specifically prepares process and may further comprise the steps successively:
Step 1, material choice:
Molybdenum powder: purity>=99.96%, loose density 0.95g/cm
3~1.40g/cm
3, granularity 2.0 μ m~3.5 μ m;
La
2O
3Powder: purity is 99.99%, and granularity is 0.5 μ m~2 μ m;
The TiH powder: purity >=99.5%, granularity are 5~8 μ m;
ZrH
2Powder: purity>=99.5%, granularity are 5~8 μ m;
Graphite Powder 99: purity >=99.5%, maximum particle size are no more than 10 μ m;
Step 2 is carried out proportioning: TiH according to following mass percent
2Powder: 0.45%~0.65%, ZrH
2Powder: 0.06%~0.14%, Graphite Powder 99: 0.02%~0.06%, La
2O
3Powder: 0.5~1.5%, surplus is a molybdenum powder, the per-cent sum of raw material is 100%;
Step 3 is packed each raw material of formula ratio in the three-dimensional blender machine into, mixes 1~4 hour the powdered alloy that obtains mixing with rotating speed 30r/min~60r/min;
Step 4 is packed powdered alloy into and is carried out ball milling in the ball mill, and drum's speed of rotation is 30r/min~200r/min, and being placed with diameter in the ball mill is the molybdenum ball of 10mm, and the mass ratio of molybdenum ball and powdered alloy is 2: 1,2 hours~24 hours ball milling time;
Step 5, the alloy powder behind the ball milling adopt mold pressing or isostatic pressing method to be pressed into blank, and pressure is 20Mpa~200Mpa, and the dwell time is 5s~60s;
Step 6 is carried out pre-burning with the blank that suppresses, and protective atmosphere is vacuum, hydrogen or rare gas element, and pre-sintering temperature is 1000 ℃~1200 ℃, is incubated 1 hour~4 hours;
Step 7 is carried out high temperature sintering with the blank after the pre-burning, and protective atmosphere is vacuum, hydrogen or rare gas element, and the highest sintering temperature is 1800 ℃~2000 ℃; High temperature sintering adopts the staged sintering processing; Promptly when being heated to 1200 ℃~1500 ℃; Whenever at a distance from 100 ℃ of insulations 2~3 hours, when being heated to 1500 ℃~1800 ℃, whenever at a distance from 150 ℃ of insulations 2~4 hours; Be incubated 5-8 hour down at 1800 ℃~2000 ℃ at last, promptly obtain thin brilliant high-compactness TZM alloy.
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CN104525948A (en) * | 2014-12-23 | 2015-04-22 | 金堆城钼业股份有限公司 | Preparation method for molybdenum alloy electrode |
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CN109332717A (en) * | 2018-09-20 | 2019-02-15 | 中国航天空气动力技术研究院 | A kind of preparation method of spherical shape molybdenum titanium-zirconium alloy powder |
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CN110270683A (en) * | 2018-03-16 | 2019-09-24 | 武汉理工大学 | A kind of Fe/ZrH2Nanocomposite particle and its preparation method and application |
CN111644632A (en) * | 2020-04-20 | 2020-09-11 | 淮北师范大学 | Preparation method of rare earth lanthanum oxide doped TZM alloy |
CN112281041A (en) * | 2020-10-16 | 2021-01-29 | 内蒙金属材料研究所 | Lutetium oxide particle reinforced molybdenum-based composite material and preparation method thereof |
CN114457248A (en) * | 2021-12-22 | 2022-05-10 | 重庆材料研究院有限公司 | Preparation method of molybdenum-ruthenium alloy wire for high-temperature brazing |
CN114657404A (en) * | 2022-03-24 | 2022-06-24 | 金堆城钼业股份有限公司 | High-density ultrafine-grained molybdenum-lanthanum alloy and preparation method thereof |
CN114951639A (en) * | 2022-05-10 | 2022-08-30 | 厦门虹鹭钨钼工业有限公司 | High-density fine-grain structure molybdenum alloy plug and preparation method thereof |
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2012
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